JPH01230481A - Production of sintered aluminum nitride - Google Patents
Production of sintered aluminum nitrideInfo
- Publication number
- JPH01230481A JPH01230481A JP63056355A JP5635588A JPH01230481A JP H01230481 A JPH01230481 A JP H01230481A JP 63056355 A JP63056355 A JP 63056355A JP 5635588 A JP5635588 A JP 5635588A JP H01230481 A JPH01230481 A JP H01230481A
- Authority
- JP
- Japan
- Prior art keywords
- aluminum nitride
- carbon
- thermal conductivity
- powder
- sintering assistant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 48
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 25
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 6
- 238000010304 firing Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 230000007423 decrease Effects 0.000 abstract description 2
- 239000002775 capsule Substances 0.000 abstract 2
- 238000001354 calcination Methods 0.000 abstract 1
- 239000006229 carbon black Substances 0.000 description 9
- 238000009413 insulation Methods 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- 229910052582 BN Inorganic materials 0.000 description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 150000001722 carbon compounds Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、窒化アルミニウム焼結体の製造方法に関する
ものである。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to a method for manufacturing an aluminum nitride sintered body.
（従来の技術）
近年、半導体素子の高集積化、高機能化が進み従来のＡ
ｌ２Ｏ３ではＳｉチ・シブの発熱量の増大、チップサイ
ズの大型化による熱膨張のミスマツチの問題への対応が
難かしく、新しい高熱伝導性絶縁材料が求められている
。(Conventional technology) In recent years, semiconductor devices have become highly integrated and highly functional.
With l2O3, it is difficult to deal with the problems of increased heat generation of Si chips and thermal expansion mismatch due to larger chip sizes, and new high thermal conductivity insulating materials are required.
窒化アルミニウム（ＡＩＮ）は高熱伝導性の他に、熱膨
張率がＳｉチップに近く、又高電気絶縁性などの優れた
材料特性を有する為、半導体装用基板材料として特に注
下を集めている。Aluminum nitride (AIN) has excellent material properties such as high thermal conductivity, a coefficient of thermal expansion close to that of Si chips, and high electrical insulation properties, so it is attracting attention as a substrate material for semiconductor devices.
ＡＩＮは難焼結性物質であるため緻密な焼結体を得るこ
とが困難である。また原料中には不純物酸素を通常１〜
３ｗｔ％程度含有しており、焼結助剤なしでホットプレ
ス等で緻密に焼結させてもＡＩＮ粒子のまわりにＡｌ−
０−Ｎなどの酸素固溶層が形成され、熱伝導率が著しく
低下することが知られている。Since AIN is a difficult-to-sinter substance, it is difficult to obtain a dense sintered body. In addition, the impurity oxygen in the raw material is usually 1~
It contains about 3wt%, and even if it is densely sintered with hot press etc. without a sintering aid, Al-
It is known that an oxygen solid solution layer such as 0-N is formed and the thermal conductivity is significantly reduced.
従来より、ＡＩＮの緻電化、高熱伝導化をはかるため、
種々の焼結助剤か検討されてきたが、これらの中でＹ２
０３ 、 ＧａＯなとの醇化物が４＋ｊに有効であるこ
とがわかってきた。（Ｐｒｏｃ、１ｓｔ ＩＥＥＥＣＨ
ＭＴ Ｓｙｍｓ、、＋５（＋９８４））例えばＹ２Ｏ３
添加による高熱伝導化の機構についてはＹ２Ｏ３か不純
物酸素と反応し、ＡＩＮ粒界の三重点にＹＡＧなとの化
合物を形成し、酸素をトランプするためと考えられてい
る。このようにＹ２Ｏ３添加により高熱伝導化は、はか
られるが、熱伝導率は約１００Ｗ／ｍｋ程度と理論値の
３２０Ｗ／ｍｋに比較して充分高いとはいいがたい。そ
の他、多数の焼結助剤が提案されているが、本発明のカ
ーボン添加に関連した従来技術についてもいくつか報告
されている。Conventionally, in order to make AIN denser and more thermally conductive,
Various sintering aids have been studied, but among these, Y2
03, It has been found that infusions with GaO are effective for 4+j. (Proc, 1st IEEECH
MT Syms, +5 (+984)) e.g. Y2O3
The mechanism of high thermal conductivity due to addition is thought to be that Y2O3 reacts with impurity oxygen, forms a compound such as YAG at the triple point of the AIN grain boundary, and trumps the oxygen. As described above, high thermal conductivity can be achieved by adding Y2O3, but the thermal conductivity is about 100 W/mk, which is not sufficiently high compared to the theoretical value of 320 W/mk. Many other sintering aids have been proposed, and some prior art related to the addition of carbon in the present invention has also been reported.
カーボンを成形体中に添加する方法については、特開昭
６Ｏ−１８Ｆ１４７９号公報、特開昭８１−１５５２６
３号公報に記載されている。前者ではＡＩＮ粉末に炭素
又は分解して炭素になる化合物を、後者ではＡＩＮ粉末
に遊＃炭素、酸化イツトリウムを添加し成形、焼成を経
て、熱伝導率がそれぞれ５０Ｗ／ｍｋ 、 １５０Ｗ／
ｍｋ程度のＡＩＮ焼結体をえている。Regarding the method of adding carbon into a molded body, JP-A No. 6O-18F1479 and JP-A No. 81-15526
It is described in Publication No. 3. In the former, carbon or a compound that decomposes into carbon is added to the AIN powder, and in the latter, free carbon and yttrium oxide are added to the AIN powder, and through molding and firing, the thermal conductivity is 50 W/mk and 150 W/mk, respectively.
An AIN sintered body of about mk is obtained.
更に特開昭８１−２７０２６３号公報ではＡＩＮ粉末に
Ｔｉなどの元素又は化合物を添加し、硼素及び／又は炭
素の供給源を有する非酸化性雰囲気中で焼成することに
より、約９０Ｗ／ｍｋの熱伝導率を有する焼結体を得て
いる。以上のようにカーボン添加に関連した系でいくつ
か報告されているが、いずれも熱伝導率は１５０Ｗ／ｍ
ｋ程度で不十分であり、更に熱伝導率の高い窒化アルミ
ニウム焼結体が求められていた。Furthermore, in JP-A No. 81-270263, an element or compound such as Ti is added to AIN powder, and by firing in a non-oxidizing atmosphere with a boron and/or carbon source, a heat of about 90 W/mk is produced. A sintered body with conductivity has been obtained. As mentioned above, several systems related to carbon addition have been reported, but all have thermal conductivity of 150 W/m.
A sintered aluminum nitride body having even higher thermal conductivity was required.
［発明の解決しようとする問題点］
本発明はカーボン添加に関連した従来技術が有していた
前述の欠点を解消しようとするものであり、熱伝導率が
２００Ｗ／ｍｋ程度の高熱伝導性窒化アルミニウム焼結
体を安定的に供給する製造方法を提供することを目的と
するものである。[Problems to be Solved by the Invention] The present invention attempts to solve the above-mentioned drawbacks of the conventional technology related to carbon addition, and uses a highly thermally conductive nitrided material with a thermal conductivity of about 200 W/mk. The object of the present invention is to provide a manufacturing method that stably supplies aluminum sintered bodies.
［問題点を解決するだめの手段］
本発明は前述の問題点を解決すべくなされたものであり
、窒化アルミニウム粉末と焼結助剤・を混合して成形し
た後、この窒化アルミニウムの成形体とカーボン供ｆＩ
＠源を少なくとも内面が非カーボン質のサヤの中に入れ
、非酸化性雰囲気中で焼成することを特徴とする窒化ア
ルミニウム焼結体の製造方法を提供するものである。[Means for solving the problem] The present invention was made to solve the above-mentioned problem, and after mixing aluminum nitride powder and a sintering aid and molding, the aluminum nitride molded body is and carbon supply fI
The present invention provides a method for producing an aluminum nitride sintered body, characterized in that a source is placed in a pod whose inner surface is at least non-carbonaceous and fired in a non-oxidizing atmosphere.
（構成の詳細説明） 以下、本発明について詳細に説明する。(Detailed explanation of the configuration) The present invention will be explained in detail below.
まず、窒化アルミニウムの粉末は高純度のもの、例えば
９８％以上のものが好ましいが、９５〜９８％程度のも
のも使用可能である。粒径は１０μｍ以下、好ましくは
２μｍ以下のものか良い。粒径か１０ｇｍをこえると焼
結性か低下し好ましくない。First, aluminum nitride powder is preferably of high purity, for example, 98% or higher, but powder of about 95 to 98% can also be used. The particle size may be 10 μm or less, preferably 2 μm or less. If the particle size exceeds 10 gm, the sinterability will deteriorate, which is not preferable.
かかる窒化アルミニウムの粉末に添加される焼結助剤は
緻密な焼結体を得るものて、Ｙ、０３゜ＣａＯなどか好
ましいか、緻密化を促進するものてあれば、これに限定
されるものではない。−方、焼結助剤の添加量か多過ぎ
ると窒化アルミニウム以外の結晶相か増加し、熱伝導率
か低下するものて好ましくない。従って、好ましい焼結
助剤の添加量は１０ｗｔ％以下、特に好ましくは５ｗｔ
％以下である。The sintering aid added to the aluminum nitride powder is preferably one that produces a dense sintered body, and is preferably Y, 03°CaO, or is limited to any agent that promotes densification. isn't it. On the other hand, if the amount of the sintering aid added is too large, crystal phases other than aluminum nitride will increase and the thermal conductivity will decrease, which is not preferable. Therefore, the amount of the sintering aid added is preferably 10 wt% or less, particularly preferably 5 wt%.
% or less.
また、焼結助剤の粒径は細かい方が好ましく、特に１戸
１１以下か望ましい。かかる窒化アルミニウム粉末と焼
結助剤を所定の割合て混合後、ドクターブレード法又は
プレス法により所定形状に成形し、Ａ１と耐素の反応に
より熱伝導率か低下するのを防ぐためにこれを窒素など
の非酸化性雰囲気中て焼成する。この際成形体は少なく
とも内面か非カーボン質のサヤに収められるか、サヤの
材質としては、常圧て窒化アルミニウム焼成温度より融
点、又は昇華分解温度の高い例えば窒化アルミニウム、
窒化ホウ素、炭化ケイ素などが望ましい。特に窒化アル
ミニウム、窒化ホウ素製のサヤは窒化アルミニウム焼結
体の焼結性、熱伝導性の向上を阻害せずより望ましい。Further, the particle size of the sintering aid is preferably fine, and particularly preferably 11 or less per unit. After mixing the aluminum nitride powder and the sintering aid in a predetermined ratio, it is formed into a predetermined shape by a doctor blade method or a press method, and then nitrogen gas is added to prevent the thermal conductivity from decreasing due to the reaction between A1 and the element. Calcinate in a non-oxidizing atmosphere such as In this case, the molded body is housed in a non-carbon sheath at least on the inner surface, or the material of the sheath is aluminum nitride, which has a melting point or sublimation decomposition temperature higher than the firing temperature of aluminum nitride at normal pressure.
Boron nitride, silicon carbide, etc. are preferable. In particular, sheaths made of aluminum nitride or boron nitride are more desirable because they do not impair the improvement of the sinterability and thermal conductivity of the aluminum nitride sintered body.
又サヤとして安価で軽く、加工性に優れたカーボンを使
用する場合は、少なくともサヤの内面を上記の窒化アル
ミニウム、窒化ホウ素などの材質でコーティングするこ
とにより、焼成時でのカーボンの遊離を押える効果をも
たせることが望ましい。In addition, when using cheap, lightweight, and easily workable carbon as the pod, coating at least the inner surface of the pod with the above-mentioned materials such as aluminum nitride or boron nitride is effective in suppressing the release of carbon during firing. It is desirable to have
更に、上記サヤ内には同時にカーボンの供給源としてカ
ーボン粉末、カーボンセラミックス、容易にカーボンに
転換しうる炭素化合物（例えば、バインダーに使用され
る炭素化合物）のうち少なくとも１つを入れる。これら
カーボン供給源にはＡＩＮ焼結体の物性を左右する適量
か存在し、供給量か不足の場合は熱伝導率は１００〜１
２０Ｗ／ｍｋ程度と低く、供給過剰になると熱伝導率は
２００Ｗ／ｍｋ程度まて向上するか絶縁抵抗は１０９〜
１０１０Ωｃｍまて劣化し、いずれも好ましくない。Further, at the same time, at least one of carbon powder, carbon ceramics, and a carbon compound that can be easily converted into carbon (for example, a carbon compound used in a binder) is placed in the pod as a carbon supply source. These carbon sources exist in appropriate amounts that influence the physical properties of the AIN sintered body, and if the supply is insufficient, the thermal conductivity will be 100 to 1.
The thermal conductivity is low at around 20W/mk, and if there is an oversupply, the thermal conductivity increases to around 200W/mk or the insulation resistance is 109~
It deteriorated by 1010 Ωcm, which is not preferable.
カーボン供給源か適量の場合、熱伝導率は２００Ｗ／ｍ
ｋをこえ、絶縁抵抗１０１４Ωｃｍ以上と良好な特性を
示す。このようにカーボン供給源の適量添加か重要てあ
り、例えば焼成時に使用するカーボンサヤ、発熱体など
の炭素をその供給源とした場合、サヤ、発熱体の形状、
表面状態、使用状態位置などによりカーボン供給量か著
しく変動し、良好な特性を有するＡＩＭ焼結体を安定的
に確保することか困難である。そのため本発明てはカー
ボンの適量添加をはかるため、前述のようにサヤの少な
くとも内面を非カーボン質として、サヤ、発熱体からの
カーボンの侵入を防止した上て、サヤ内に適量のカーボ
ン供給源を入れる方法を採用した。In case of carbon source or proper amount, thermal conductivity is 200W/m
It exhibits good characteristics with an insulation resistance of 1014 Ωcm or more. In this way, it is important to add an appropriate amount of carbon source.For example, when carbon is used as a source of carbon such as a carbon pod or heating element used during firing, the shape of the pod or heating element,
The amount of carbon supplied varies significantly depending on the surface condition, position of use, etc., and it is difficult to stably secure an AIM sintered body with good characteristics. Therefore, in the present invention, in order to add an appropriate amount of carbon, at least the inner surface of the pod is made non-carbonaceous to prevent carbon from entering from the pod and the heating element, and an appropriate amount of carbon is added within the pod. We adopted the method of adding .
組成中にすてにカーボンを添加する方式についても実験
を行なったか、熱伝導率は１５０Ｗ／ｍｋ程度までしか
上からなかった。An experiment was also conducted on a method in which carbon was already added to the composition, and the thermal conductivity increased only to about 150 W/mk.
［作用］
本発明てはサヤ内にカーボン供給源を適量添加すること
により熱伝導率か著しく向上することを見い出した。こ
の高熱伝導化のメカニズムについてはまた明らかてはな
いか、サヤに入れる窒化アルミニウム成形体の重量とと
もに最適なカーボン量も増加する傾向にあることや、−
般にＡＩＮの高熱伝導化に不純物酸素か密接に関連して
いることから、成形体中に含まれる不純物酸素かサヤ内
にカーボンを適量入れることにより、焼結過程で結果的
に粒界の三重点などにトラップされるか又は系外に除去
されるために高熱伝導化か達成されたものと考えられる
。[Function] In the present invention, it has been discovered that the thermal conductivity can be significantly improved by adding an appropriate amount of a carbon supply source into the pod. The mechanism behind this high thermal conductivity is not yet clear, and it is known that the optimal amount of carbon tends to increase with the weight of the aluminum nitride molded body placed in the pod.
In general, impurity oxygen is closely related to high thermal conductivity of AIN, so by adding an appropriate amount of carbon to the impurity oxygen contained in the molded body or the shard, three grain boundaries can be improved during the sintering process. It is thought that high thermal conductivity was achieved because it was trapped in a focal point or removed from the system.
したかって、最適なカーホン量は窒化アルミニウム成形
体の重量たけてなく、窒化アルミニウム原料に含まれる
不純物酸素量、焼成助剤の種類とその量、工程中に混入
する不純物、パインターなどの成形助剤の種類とその量
、焼成温度などに依存することか考えられる。Therefore, the optimal amount of carphone depends on the weight of the aluminum nitride molded body, the amount of impurity oxygen contained in the aluminum nitride raw material, the type and amount of firing aid, impurities mixed in during the process, and shaping aids such as painter. It is conceivable that this depends on the type and amount of carbon dioxide, the firing temperature, etc.
［実施例１］
平均粒径か２ｇｍの窒化アルミニウム粉末にＹ２０：ｌ
粉末を２．５ｗｔ％添加し、アルコール中で湿式混合し
た。次いて乾燥後２ｔノＣｌ１１２の圧力て７０ｘ ７
０Ｘ ３ ｍｍの形状に成形した。この成形体を１個、
窒化アルミニウムのサヤ（内寸法１００ Ｘ １００
Ｘ ２０ｍｍ）の中に収容し、そのまわりにカーボンブ
ラック粉末を敷き、サヤにフタをした状態で窒素雰囲気
下１８５０°Ｃで５時間保持して窒化アルミニウム焼結
体を得た。この窒化アルミニウム焼結体について相対密
度、熱伝導率、絶縁抵抗を測定した。第１表にカーボン
ブラック粉末の添加量及び測定結果を示す。試料ＮＯＩ
、２はカーボン捺加量が少なく熱伝導率は１５０Ｗ＃ｎ
ｋ以下と低かったのに対し試料Ｎｏ５，６てはカーボン
か過剰添加となっており、絶縁抵抗の劣化かみられた。[Example 1] Y20:l was added to aluminum nitride powder with an average particle size of 2 gm.
2.5 wt% of powder was added and wet mixed in alcohol. Then, after drying, the pressure of 2 tons of Cl112 was 70x7.
It was molded into a shape of 0x3 mm. One of this molded body,
Aluminum nitride pod (inner dimensions 100 x 100
The aluminum nitride sintered body was obtained by placing carbon black powder around the pod and holding it at 1850° C. for 5 hours in a nitrogen atmosphere with the pod covered. The relative density, thermal conductivity, and insulation resistance of this aluminum nitride sintered body were measured. Table 1 shows the amount of carbon black powder added and the measurement results. Sample NOI
, 2 has a small amount of carbon printing and a thermal conductivity of 150W#n
On the other hand, samples Nos. 5 and 6 had an excessive amount of carbon added, and deterioration of insulation resistance was observed.
一方試料３，４ては熱伝導率は２００Ｗ／ｍｋ前後にな
り、絶縁抵抗も１０１４Ω・ｃｍ以上と良好な結果か得
られた。On the other hand, in Samples 3 and 4, the thermal conductivity was around 200 W/mk, and the insulation resistance was also 10 14 Ω·cm or more, giving good results.
［実施例２コ
Ｙ２Ｏ３粉末のかわりにＣａＯを１．５ｗｔ％添加した
他は実施例１と同様な方法て焼成し、窒化アルミニウム
焼結体を得た。第２表にカーボンブラック粉末の添加量
及び測定結果を示す。Ｙ２Ｏ３を添加した系と同様の傾
向を示し、カーボンブラック粉末の適量添加となってい
るＮｏ９，１０ては熱伝導率、絶縁抵抗ともに良好な特
性を有していた。[Example 2] An aluminum nitride sintered body was obtained by firing in the same manner as in Example 1 except that 1.5 wt% of CaO was added instead of Y2O3 powder. Table 2 shows the amount of carbon black powder added and the measurement results. It showed the same tendency as the system to which Y2O3 was added, and Nos. 9 and 10, in which an appropriate amount of carbon black powder was added, had good characteristics in both thermal conductivity and insulation resistance.
［実施例３］
実施例１において窒化アルミニウムのサヤのかわりに内
面を窒化ホウ素てコーチインクしたカーボンサヤ（内寸
法圓Ｏｘ １００ ｘ ２０ｍｍ）を用いた以外は同様
な方法て実験を行なった。力−ボンフラック粉末の添加
量及び測定結果は下記のとおりてあった。[Example 3] An experiment was carried out in the same manner as in Example 1, except that instead of the aluminum nitride sheath, a carbon sheath (inner dimensions Ox 100 x 20 mm) whose inner surface was coated with boron nitride was used. The amount of added Bonfrac powder and the measurement results are as follows.
カーボンブラック添加量： ０．４’ｇ相対密度：
’ ９９．２％熱伝導率：
２３０Ｗ／ｍｋ絶縁抵抗：
７ Ｘ １０”Ωｃｍこのように内面を窒化ホウ素で
コープインクしたカーボンサヤを用いても良好な特性か
得られた。Carbon black addition amount: 0.4'g Relative density:
'99.2% thermal conductivity:
230W/mk insulation resistance:
7.times.10" .OMEGA.cm Good characteristics were obtained even by using a carbon sheath whose inner surface was coated with boron nitride cope ink.
［比較例１コ
実施例１て用いたＡＩＮ、Ｙ２Ｏ３，カーボンブラック
粉末を第３表に示す組成て混合し、同様に７０ｘ ’ｙ
ｏｘ ３ ＋ｎｍに成形した。この形成体のまわりにカ
ーボンブラック粉末を敷かずに１他の条件については実
施例１と同様焼成を行なった。第３表にその測定結果を
示す。[Comparative Example 1] The AIN, Y2O3, and carbon black powders used in Example 1 were mixed with the composition shown in Table 3, and 70x'y was prepared in the same manner.
It was molded to ox 3 +nm. Firing was carried out in the same manner as in Example 1 except for the fact that carbon black powder was not spread around the formed body. Table 3 shows the measurement results.
熱伝導率は実施例１に比較し、１５０Ｗ／ｍｋ程度しか
なく、相対密度も低下していた。Compared to Example 1, the thermal conductivity was only about 150 W/mk, and the relative density was also lower.
［比較例２］
実施例１において窒化アルミニウムのサヤのかわりにカ
ーボンサヤ（内寸法Ｊｏｎ ｘ １００ ｘ２〔）〕を
用い、それ以外の条件は実施例１と同様に実験をイＩな
った。カーボンブラック粉末の添加品及びＡ１１定結果
を第４表に示す。[Comparative Example 2] The experiment was carried out in the same manner as in Example 1, except that a carbon pod (inner dimensions: Jon x 100 x 2 [)] was used instead of the aluminum nitride pod in Example 1. Table 4 shows the carbon black powder additives and A11 results.
試料Ｎｏ１９はカーボンサヤ内にカーボンブラック粉末
を敷いていないにもかかわらずカーボンサヤからカーボ
ンか過剰に供給されたため絶縁抵抗か劣化しており、熱
伝導率、嵩密度も低かった。Sample No. 19 had deteriorated insulation resistance and low thermal conductivity and bulk density because carbon was supplied in excess from the carbon pod even though carbon black powder was not spread inside the carbon pod.
第１表
第２表
第３表
第４表
［発明の効果］
本発明により製造した窒化アルミニウム焼結体は高密度
で２００Ｗ／ｍｋ前後と熱伝導性に優れ、良好な電気特
性を示すことから半導体装用基板、各種ヒートシンクと
してのみならず、ルツボ、蒸着用容器、耐熱シフ高温部
材等の高温材料としての応用も可能てあり、工業的に多
くの利点を有するものである。Table 1 Table 2 Table 3 Table 4 [Effects of the Invention] The aluminum nitride sintered body produced according to the present invention has a high density and excellent thermal conductivity of around 200 W/mk, and exhibits good electrical properties. It can be applied not only as semiconductor substrates and various heat sinks, but also as a high-temperature material such as crucibles, vapor deposition containers, and heat-resistant sifter high-temperature members, and has many industrial advantages.
代理人（弁理士）平イニ１４・１」才Agent (patent attorney) 14.1 years old
Claims (1)
した後、この窒化アルミニウムの成形体とカーボン供給
源を少なくとも内面が非カーボン質のサヤの中に入れ、
非酸化性雰囲気中で焼成することを特徴とする窒化アル
ミニウム焼結体の製造方法。(1) After mixing and molding aluminum nitride powder and a sintering aid, the aluminum nitride molded body and a carbon source are placed in a sheath whose inner surface is at least non-carbonaceous,
A method for producing an aluminum nitride sintered body, which comprises firing in a non-oxidizing atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63056355A JP2661113B2 (en) | 1988-03-11 | 1988-03-11 | Manufacturing method of aluminum nitride sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63056355A JP2661113B2 (en) | 1988-03-11 | 1988-03-11 | Manufacturing method of aluminum nitride sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01230481A true JPH01230481A (en) | 1989-09-13 |
| JP2661113B2 JP2661113B2 (en) | 1997-10-08 |
Family
ID=13024935
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63056355A Expired - Fee Related JP2661113B2 (en) | 1988-03-11 | 1988-03-11 | Manufacturing method of aluminum nitride sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2661113B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002533551A (en) * | 1998-12-23 | 2002-10-08 | デグサ アクチエンゲゼルシャフト | Doped carbon black |
| WO2005123627A1 (en) * | 2004-06-21 | 2005-12-29 | Tokuyama Corporation | Nitride sintered compact and method for production thereof |
| US7737065B2 (en) | 2004-03-29 | 2010-06-15 | Denki Kagaku Kogyo Kabushiki Kaisha | Process for producing aluminum nitride sintered compacts |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59207882A (en) * | 1983-05-12 | 1984-11-26 | 株式会社東芝 | Manufacture of aluminum nitride sintered body |
| JPS62252374A (en) * | 1986-04-24 | 1987-11-04 | 株式会社村田製作所 | Manufacture of aluminum nitride sintered body |
| JPS63277573A (en) * | 1987-05-08 | 1988-11-15 | Toshiba Corp | Production of sintered aluminum nitride having high thermal conductivity |
-
1988
- 1988-03-11 JP JP63056355A patent/JP2661113B2/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59207882A (en) * | 1983-05-12 | 1984-11-26 | 株式会社東芝 | Manufacture of aluminum nitride sintered body |
| JPS62252374A (en) * | 1986-04-24 | 1987-11-04 | 株式会社村田製作所 | Manufacture of aluminum nitride sintered body |
| JPS63277573A (en) * | 1987-05-08 | 1988-11-15 | Toshiba Corp | Production of sintered aluminum nitride having high thermal conductivity |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002533551A (en) * | 1998-12-23 | 2002-10-08 | デグサ アクチエンゲゼルシャフト | Doped carbon black |
| JP4822306B2 (en) * | 1998-12-23 | 2011-11-24 | エボニック カーボンブラック ゲゼルシャフト ミット ベシュレンクテル ハフツング | Doped carbon black |
| US7737065B2 (en) | 2004-03-29 | 2010-06-15 | Denki Kagaku Kogyo Kabushiki Kaisha | Process for producing aluminum nitride sintered compacts |
| WO2005123627A1 (en) * | 2004-06-21 | 2005-12-29 | Tokuyama Corporation | Nitride sintered compact and method for production thereof |
| KR100912641B1 (en) * | 2004-06-21 | 2009-08-17 | 가부시끼가이샤 도꾸야마 | Nitride sintered compact and method for production thereof |
| US7876053B2 (en) | 2004-06-21 | 2011-01-25 | Tokuyama Corporation | Nitride sintered body and method for manufacturing thereof |
| US7973481B2 (en) | 2004-06-21 | 2011-07-05 | Tokuyama Corporation | Nitride sintered body and method for manufacturing thereof |
| JP4937738B2 (en) * | 2004-06-21 | 2012-05-23 | 株式会社トクヤマ | Nitride sintered body and manufacturing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2661113B2 (en) | 1997-10-08 |
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